FR2517325A1 - PREPARATION OF POWDERS CONTAINING ALCOHOL - Google Patents

Abstract

PROCESS FOR PREPARING WATER-SOLUBLE ALCOHOL-CONTAINING POWDERS. IT CONSISTS OF MIXING, WITH AN AQUEOUS SOLUTION CONTAINING ALCOHOL, A HYDROLYZED STARCH COMPRISING AT LEAST 50 OF OLIGOSACCHARIDES HAVING A DEGREE OF GLUCOSE POLYMERIZATION NOT EXCEEDING 8, AND AT MOST 10 OF SACCHARIDES HAVING A DEGREE OF GLUCOSE POLYMERIZATION EQUAL OR LESS THAN 2, THEN SPRAY DRYING THE RESULTING LIQUID MIXTURE. WE THUS OBTAIN, WITH A HIGH ALCOHOL YIELD RATE, EXCELLENT POWDERS WITH HIGH ALCOHOL CONTENT.

Description

The present invention relates to a process for the preparation of powders

  containing alcohol, having a high alcohol content, good solubility in

  water, a pleasant flavor and great stability to the environment.

  storage, with a high rate of alcohol yield. The conventional process of powdering a

  aqueous solution of alcohol as a liquor (alcoholic drink

  lique) consists in mixing an aqueous solution of a

  cool of appropriate concentration with a relative amount

  large amount of a water-soluble coating substance such as solid maize syrup, soluble starch, modified starch, gelatin, gum arabic or (CMC) sodium carboxymethyl cellulose, and spray-drying the powder

  containing alcohol, thus obtained, does not form a wood-

  its alcoholic only by dissolution in cold or hot water just before absorption In addition, this powder is widely used for the production of cakes and industrially cooked food In Japan, such a powder, containing alcohol, is classified as "liqueur powder" (Funmatushu) in accordance with spirits taxation regulations and is treated as a kind

of liquor.

  When preparing this alcohol-containing powder, it is necessary to obtain an excellent product with regard to solubility in water, viscosity (stickiness), flavor (flavor, fragrance and similar coating substance), resistance to moisture absorption and resistance to

  in powder form at the same time, it was born

  necessary that the alcohol content in this powder be

  the alcohol rate of return, the rate of

  duane in alcohol, is also high, in order to make the process of preparation economically and commercially advantageous. However, in this conventional process, to bring together

  all these properties, we have to overcome different diffe-

  In addition, this process proves defective in that, during the powdering of an aqueous solution of an alcohol containing a perfumed constituent, such as a liquor, not only the rate of alcohol yield

  is low, but also the residual rate of

killing scented.

  The plaintiff had tried to prepare powders containing alcohol, with a high alcohol content

  and with a high rate of alcohol yield, thanks to the

  hydrolysed starches of which 1 'E D had a

  set them, to overcome the above defects; Satisfactory results have not been obtained, including lot-specific differences in the rates of return.

  For example, when preparing different

  hydrolyzed donations to ED = 18 (value considered to be

  preferable for the experiment), and which is prepared for

  from these starches, powders containing alcohol,

  notes, although EDs are identical for

  hydrolyzed donations, discrepancies not only for the

  alcohol yield rate, but also in the

  products such as solubility and flavor.

  The present invention is based on the observation

  in subsequent studies to eliminate these difficulties, apart from the ED index, which

  the quality of a powder containing alcohol is

  the degree of polymerization of glucose, and that if

  a hydrolysed starch containing oligosaccharides is used.

  wrinkles with appropriate degrees of glucose polymerization, one can obtain, with a high rate of alcohol yield,

  a powder containing alcohol of excellent quality.

  The new process according to the invention, for the preparation of powders containing alcohol, consists of

  to mix a hydrolysed starch, comprising at least 50% of

  ligosaccharides of degree of glucose polymerization al-

  up to 8, and not more than 10% saccharides with a degree of glucose polymerization up to 2, in a solution

  aqueous solution containing alcohol and then drying this mixture

resulting equation by atomization.

  Preferably, a hydrolysed starch containing

  closing up to 5% of saccharides with a polymer

  glucose level does not exceed 2, and up to 50% of a polysaccharide whose degree of glucose polymerisation

  is greater than 9, i.e. hydrolysed starch,

  taking at least 40% of oligosaccharides with a degree of

  glucose polymerization is between 3 and 8, and the

  hydrolysed midon, so chosen, is incorporated and mixed with an aqueous solution of an alcohol whose alcohol concentration is at least 40% by weight, in an amount at least equal to 120%, relative to the water contained in the solution

  In the present description, all the

  alcohol concentrations are expressed as a percentage of

  The symbol "G" represents glucose and the number thus suffix indicates the degree of polymerization, for example, G 1, G 2 and G 3 represent respectively glucose, maltose and maltotriose, and Gn denotes saccharides the degree of

  of glucose polymerization is at least equal to 9.

  In addition, saccharides with a degree of polymerization of

  equal to or less than 2 and the oligosaccharides of which

  degree is equal to or less than 8 include G 1 (glucose).

  Oligosaccharides are usually not

  present in free form in their natural state, and they are

  by acidic or enzymatic hydrolysis of amylose, amyloid

  lopectin or glycogen An oligosaccharide formed by hy-

  partial drolysis of a starch, using an acid or an enzyme, has a "-1,4 bond, sometimes with a small amount of" 1,6-bond. The results of the determination of the properties of the saccharide composition of commercially hydrolysed starches are shown in Table 1, on page 21

  The ED index is usually adopted as the index of

  the degree of hydrolysis of a starch, and it is often

  used as a factor of discernment of the mass of

  the average sweetness potency, the viscosity and the moisture absorption capacity However, as the ED index is calculated in relation to the results of measurements made on a direct reducing sugar of a hydrolysed starch, the Characteristics of the saccharide composition or the properties of the hydrolysed starch can not be strictly expressed by the ED index. For example, as the mechanism of acid hydrolysis differs

  considerably from that of enzymatic hydrolysis,

  if the ED indices are similar, the composition of

  hydrolysed starch saccharides obtained by acid hydrolysis

  differs from that of the product which hydrolysis gives

  zymatic properties, and the properties of the two different hydrolysates

  rent. It is apparent from Table 1 that it is practically impossible to presume the saccharide composition of the hydrolysed starch from the ED number. It is seen that a hydrolysed starch used in the present invention

  which comprises at least 40% oligosaccharides, degree / po-

  glucose lymerization from 3 to 8, and up to 10% saccha-

  wrinkles with a degree of glucose polymerization equal to or less than 2, are not included in the available products

Trade.

  Hydrolysed starch, used in accordance with the

  vention, which comprises up to 10% lower saccharides with a degree of glucose polymerization equal to or less than

  2, and up to 50% of polysaccharides having a degree of

  glucose lymerization equal to or greater than 9, i.e.

  at least 40% of oligosaccharides at the degree of polymerisation

  glucose level of 3 to 8, is prepared according to

  As described above, hydrolysed starches, obtained by other methods, can be used if the desired objectives of the present invention can be achieved.

  to be reached by this use.

  (1) A process comprises the fractionation of a

  starch obtained by conventional, acid or enzymatic hydrolysis

  that hydrolysed starch containing oligosaccharides

  G 3 to G 8 at levels as high as possible; we pre-

  fers hydrolysed starch mainly by enzymatic

  that having an ED number of 15 to 30 The fractionation is carried out with the aid of an alcohol, and is followed by the separation and the elimination of the useless constituents,

  to obtain a hydrolyzed starch of the saccharide composition

charides mentioned above.

  (2) Another process involves subjecting a starch to special liquefaction in 2 stages, using

  of the amylase giving a hydrolysed starch of the

  saccharide position indicated above.

  According to the conventional technique, it is very difficult to obtain only a product of degree of polymerization

  by a reaction using an acid and O-amine

  lase, but recently (1972-1973) a process was developed

  for obtaining a hydrolysed starch, a main compound

  oligosaccharides and having reduced levels of glucose and maltose, by special liquefaction in 2 stages, with o-amylase having the particularity of being

  able to selectively hydrolyze relatively

large.

  (3) A third method includes conversion

  biochemistry (digestion and elimination) of saccharides

  G and G 2, contained in a hydrolysed starch; it is preferable to use a hydrolyzed starch containing oligosaccharides G 3 to G 8 at levels as high as possible and reduced contents of saccharides G 9 to G n, the conversion takes place using a microorganism such as

than yeast.

  (4) In another process a reaction is made

  liquefied starch with an enzyme generating malt-oligomer

  saccharide, as a malt-pentose-generating enzyme, and the resulting hydrolysed starch having a high maltoligosaccharide content is treated according to the method (1) or (3) above; it can be used directly if its

  saccharide position is within the range

diqué above.

  In these processes, ordinary starches, such as maize, potato, or tapioca, as well as starch substrates, are initially used, such as

  amylose, amylopectin and glycogen.

  In the process for the preparation of powders containing alcohol, according to the present invention, it is possible to use, in addition to the hydrolyzed, specific starch,

  defined above, a coating substance or vehicle, such as

  gelatin, gum arabic or CMC, provided that the characteristics of the process according to the invention are not lost.

  Hydrolysed starch, which is used according to

  invention, must satisfy the basic requirement

  that the content of oligosaccharides, of degree of polymerisation

  glucose level equal to or less than 8, ie at least 50%,

  and that the saccharide content, including that degree of polymerisation,

  sation is equal to or less than 2, ie less than 10%.

  However, it is preferable that the saccharide content, with a degree of polymerization of glucose equal to or less than

  2, does not exceed 5%; when using such a hyaline starch

  drolysed, the rate of alcohol yield can be further improved. It is preferred that the hydrolyzed starch used in the present invention is soluble in a

  aqueous solution of an alcohol at 40% w / w; this if-

  that if a 25% aqueous solution of the

  drolyzed is added to a 40% w / w

  weight of an alcohol (250 C), at the rate of 5% in relation to

  the absorption capacity (absorbance) of the mixture

  at 600 nm, after 5 minutes, is less than 0.5.

  critical soluble treatment of hydrolysed starch in

  cool is determined according to the degree of polymerization and the amount of a high polymer portion of the hydrolysed starch as can be seen from the results

  obtained in the test described hereinafter, when the hydrophilic starch

  The polysaccharide is soluble in an aqueous alcohol solution at minus 40% w / w, it can be added and mixed with an aqueous solution of high alcohol concentration, and it is possible to prepare a high-grade powder.

  in alcohol, with a high rate of return in it.

  In accordance with the present invention,

  pore in an aqueous solution containing alcohol,

  a hydrolysed starch comprising at least 50% oligosaccharide

  wrinkles with equal or lower glucose

  8 and up to 10% of saccharides with such a degree

  equal to or less than 2; the resulting liquid mixture is dried

both by atomization.

  In particular, as an aqueous solution

  with alcohol, malt liquors (fermented liqueurs

  such as wine and refined "sake", spirits such as whiskey, brandy, rum and "shochu", mixed liquors such as

  "mirin", herb-based spirits, liqueurs of

  seasoning as wine and "mirin" rendered un drinkable, perfumes such as vanilla tincture or orange essence, tinctures of spices such as pepper, ginger

  raw drugs such as liquorice root, gentian root

  green extracts of aqueous alcohol

  tablecloths such as tea leaves, coffee beans and

  of cocoa, extracts of aqueous alcohol from products of

  seasoning such as seaweed and bonito, and their mixtures.

  The hydrolysed starch is added to an aqueous solution containing at least 20% w / w of alcohol, and preferably more than 40% w / w, in an amount of 100 to 200%, based on the water contained in the solution. aqueous alcohol, then the resulting liquid mixture is dried

by atomization.

  According to the method according to the invention

  As mentioned above, high alcohol content yields a variety of high grade powders.

in alcohol.

  The test according to the present invention is described below.

TRIAL

  Α-Amylase is added to a corn starch emulsion, and the hydrolysis is conducted to an ED of 8%.

  hydrolysis liquid is heated at 130 ° C. for 10 minutes.

  and then cooled down: "-amylase is added again

  and the hydrolysis is carried out to an ED of 21.5.

  The analytical results of the hydrolysed starch, obtained before fractionation, are given in Table 2, on page 22. To 200 kg of a 58% aqueous solution of alcohol, 100 kg of a dry product of 100 ml are added. hydrolysed starch obtained, which gives an opaque liquid mixture.

  this mixture for 12 hours, to obtain 2 trans-

  relatives; the upper layer, separated and dried, gives the fraction A. 130 kg of a

  aqueous solution containing 47% alcohol, which leads to a

  liquid, opaque lange left for 12 hours, this

  mixture gives 2 transparent layers The upper layer

  re, separated and dried, constitutes the fraction B, and the

  lower, dried, fraction C The analytical results

  of the 3 fractions, thus obtained, are indicated in

Table 2.

  With the fractions A, B and C, as well as with a mixture of 1/3 of the fractions A and C and hydrolysed starch before fractionation, liquid mixtures (40 C), which differ in the amount of alcohol relative to the water and the amounts of saccharides relative to water, as shown in Tables 3 to 7 Each liquid mixture is heated to 600 C with a plate, then spray dried to a room temperature of 750 C. The powders containing alcohol are thus obtained

  In addition, liquid mixtures are prepared, indi-

  in Table 8, using glucose, maltose

  (including 95% maltose and 5% glucose) and maltotrio-

  se (comprising 90% maltotriose and 5% maltohexose) commercially available, prepared by hydrolysis of pullulan (Pullulan PF-10 Hayashibara K K) with the aid of pullulanase (CK 20-L Amano Seiyaku K K); each

  liquid mixture is spray-dried at a temperature of

  room temperature of 750 C The results obtained are indi-

Table 8.

  (See Tables 3 to 8 on pages 23 to 28) In Tables 3 to 8, each% represents the

  alcohol content of the powder, and each% in parentheses

  corresponds to the alcohol yield.

  In Tables 5 and 6, the "white haze" indicates that the coating substance (vehicle) is not dissolved in the aqueous alcohol, and that there is separation in the liquid mixture. white A "indicates that

  an abundant white cloud is observed, and there is immediate

  separation of the liquid mixture into 2 layers, the "white cloud C" indicates that the white cloud is observed that there is hardly any separation, and the "white cloud"

  B "means an intermediate state between the 2 previous ones.

  These liquid mixtures are spray dried under stirring.

sufficient.

  In the course of carrying out this invention,

  composition, saccharide composition, viscosity,

  soluble, critical concentration, in alcohol and performance

  alcohol, are determined and calculated according to the following

  solvents. Saccharide composition: it is qualitatively determined by chromatography

  using the PNH 2-10 / 52504 column (provided by Shi

  mazu Seisakusho), a water-acetonitrile mobile phase, and a

  differential diffractometer as a detection device.

  Viscosity: in 500 g a sample of 500 g / water is dissolved, and the viscosity is measured at 40 C with a rotary viscometer of the type

cylindrical.

  Concentration soluble, critical, in alcohol:

  aqueous solutions of alcohol of different colors are prepared at 25 ° C.

  different concentrations; 10 ml of each is poured into a test tube and added to each

  0.5 ml of a 25% aqueous solution of the sample

  lon; after 5 minutes, we measure the abil-

  sorption at 600 nm; the results obtained are reported

  on a graph, and the concentration of the aqueous solution

  of alcohol, giving the absorption capacity of 0.5, is

  noted and defined as the soluble, critical concentration.

  Use rate of alcohol: the alcohol yield is calculated according to the following formula

B 100

  yield of alcohol (%) = x Ex 1 AO in which A is the quantity of alcohol used, B the amount of saccharides used (solids), C that of saccharides% (solids) contained in the powder containing alcohol, produced, D the quantity (%) of water contained

  in this powder, and E the alcohol content (%) in this

powder.

  G 1, G 2, G 3, Gn correspond to the saccharides having

  respective degrees of glucose polymerization

at 1, 2, 3, n.

  As can be seen from Table 3, when using fraction A, which contains G 1 and G 2

  exceeds 30%, although it can be added in large quantities

17325

  to high-alcohol aqueous solutions of alcohol

  alcohol, and in large quantities in relation to the water

  in alcoholic aqueous solutions, the yield of alcohol is very low. As can be seen in Table 5, when fraction C is used,

  in polysaccharides at G> 9 exceeds 80%, the concentration

  in alcoholic solubles is low and the fraction

  C is insoluble in a concentrated aqueous solution.

  high in alcohol: the viscosity is then very large and the amount dissolved in the water small Therefore, even if the object sought is to obtain a high content of

  alcohol and a high rate of alcohol yield, such as

  mixed, prepared, has a white cloud and

  paration, or can not be spray-dried because of

  too much viscosity, it proves impossible to pre-

  On the other hand, when the concentration of alcohol is low, and the amount of fraction C compared to water, the yield of

  alcohol and the alcohol content, obtained, are not less than

  those obtained when using fraction B (see Table 4), when the added amount of fraction B and the alcohol concentration are identical to those described above, but can not be obtained

  a powder with a high alcohol content with a

  alcohol is high. It is apparent from the experimental data

  (see Table 6) for mixing in the proportion

  of 1/3 of the fractions A and C, that, although the degree of

  average polymerization of the mixture is virtually identical

  than that of fraction B, the harmful influences of the low saccharides G 1 and G 2 and the polysaccharides Gn are

  that is why the alcohol yield is low.

  ble and it is impossible to prepare a product with a

  high alcohol content Based on experimental data

* Table 8 shows that maltotriose (G 3) has

  alcohol coating properties, and that the low saccharides

  wrinkles <G 1 and G 2) have practically none, and that in -

  the case of these low saccharides, powdering is very difficult. From the previous experimental data, it can be seen that among the constitutive saccharides of the hydrolyzed starches, those having a degree of glucose polymerization of at least 3, have a coating capacity of the alcohol, that the low saccharides G 1 and G 2 hardly have it,

  and the powdering of these is very difficult.

  It appears from the data in Tables 3 to 7 that, if the

  coating substance (vehicle) is strong,

  with water (and the aqueous solution of alcohol), the

  alcohol is increased.

  that if the concentration of the vehicle is increased,

  the alcohol content in the resulting powder is decreased.

  It thus becomes evident that, in order to prepare a powder with a high alcohol content with a high yield, it is necessary to add a high concentration vehicle to an aqueous solution with a high concentration of alcohol.

  polysaccharides with a higher degree of glucose polymerisation

  at about 9 have sufficient powers of alcohol coating, but as the degree of polymerization increases, it becomes difficult to dissolve in an aqueous solution of high alcohol concentration and

  high concentration water (because of the high

  cosity). It is therefore clear that polysaccharides

  of, having a glucose polymerization degree greater than about 9, are not suitable for producing powders

  high alcohol content, with a high yield.

  In general, from the above experimental data, when a hydrolysed starch is selected according to

  criteria set out above, in the definition of the invention

  and spray-dry the liquid mixture

  At a temperature as low as possible, it is possible to obtain a powder containing a high alcohol content, with a high yield therein; solubility in 1 '

  water of the powder thus obtained is very good and the

  In addition, the sweetening power of this powder attributable to the coating substance is low, and a large number of its

  properties, in powder form, as resistance to absorption

  humidity, resistance to caking, and

  perfume retention, are excellent In conclusion

  in the case where the composition of the saccharides is

  ve in the interval mentioned above, as the content of oligosaccharides G 3 to G 8 increases, the properties of the

  powder containing alcohol can be improved.

  In accordance with the present invention, not only the

  In addition to the alcohol content, various scented components can be simultaneously powdered. It has been found that the residual content of low-boiling scented constituents is similar to that of the alcohol.

  practically proportional to the alcohol yield

  follows that, to obtain a powder containing liquor alcohol, or the like, retaining perfumed constituents,

  it is important to increase the alcohol yield.

  The present invention is described in detail with

  reference to the following nonlimiting examples.

EXAMPLE 1

  300 kg of an aqueous solution containing 63% of alcohol are added with stirring 150 kg of a hydrolyzed starch (ED number = 24 and water content of 5%), the composition of which is: 7, 8% G 1, 7.7% G 2, 8.6% G 3, 8.2% G 4, 7.5% G 5, 7.2% G 6, 6.4% G 7, 7.5% G 8, and 39.1% Gn; we get a

  opaque liquid mixture This liquid is allowed to stand

  15 hours, until separation into 2 transparent

  Fractionation gives 205 kg of a layer greater than 13.8% solids, 58.5% alcohol and 27.7% solids.

  water, as well as 245 kg of a lower layer with

  in solid 46.5%, alcohol 28.2% and water, 3%. To the 245 kg of the bottom layer, 5 kg of water are added, and the resulting liquid mixture is heated to 60 ° C using

  of a hot plate and spray-dried at a time

  room temperature of 75 ° C., which gives about 180 kg of a powder having an alcohol content of 35% and water of 3% (the yield of alcohol is 93%). The powder thus obtained is highly soluble in water, and its solution

  water has a sweetening power and a viscosity re-

  duits, a good flavor; it is very stable to conserva-

  Thus, it is found that this powder is of interest

  as a powdered cocktail or as a pastry additive

  series and the like The saccharide composition of the alcohol-containing powder obtained comprises 2.6% G 1, 2.8% G 2, 7.4% G 3, 8.6% G 4 , 8.5% of G 5, 8.4% of G 6,

  7.5% G 7, 8.8% G 8 and 45.4% Gn.

  When distilling the separate upper layer,

  an aqueous solution of 65% alcohol is obtained.

  It can be used repeatedly for the above-mentioned fraction. The composition of the distillation residue

  includes: 28.5% G 1, 27.3% G 2, 13.5% G 3, 6.7% G 4, 3.3% G 5, 2.7% G 6, 2.2% of G 7,

2.3% of G 8 and 13.5% of Gn-

EXAMPLE 2

  It is mixed and dissolved in 300 kg of an aqueous solution of

  58% alcohol, 190 kg of a hydrolysed starch (ED = 23 and

  5% in water) whose saccharide composition is: 7.1% G 1, 7.3% G 2, 7.8% G 3, 8% G 4, 6.8% G 5, 7.2% of G 6, 6.8% of G 7, 8.1% of G 8 and 40.9% of Gn, and as described in Example 1, the liquid mixture is separated into

  an upper layer (A) of 190 kg and a lower layer

  re (B) 300 kg The top layer (A) has a solids content of 28.5%, alcohol 47.9% and water 23.5%; the lower layer (B) contains 42.4% solids, 27.3%

  alcohol and 30.3% of water The 300 kg of the lower layer

  re (B) are subsequently mixed with 167 kg of alcohol

  92.4% and 133 kg of water and, as in Example 1, the

  The liquid mixture is separated into an upper layer (C) of 382 kg and a lower layer (D) of 218 kg. The upper layer (C) has a solids content of 19.8%, alcohol of 41.4% and 38.8% water: the lower layer (D) con-

  holds 23.6% solids, 35.9% alcohol and 40.4% water.

  As described in Example 1, the constituent

  cool is collected from the 382 kg of the top layer

  (C) and the residue is dried to give 75 kg of a dry product (5% water) CO produced with the saccharide composition: 2.7% G 1, 2.8% G 2, 6.3% G 3, 8.9% G 4, 9.5% G 5, 9.8% G 6, 11.2% G 7, 12% G 8 and 36.8% of Gn, and the critical alcoholic concentration is

  of 52%, the viscosity of 23 cps and the ED index of 17.1.

  50 kg of the dry product obtained are then mixed and dissolved.

  65 kg of an original "Scotch whiskey" with an alcohol content

  cool 48%, and the liquid mixture, obtained, is heated to C with a plate, and dried at a chamber temperature of 70 C, which gives about 78 kg of a Scotch whiskey powder to 36% alcohol content (91% alcohol yield) Scented constituents, other than alcohol, are recovered, virtually without loss, together with

  alcohol When this powder is dissolved in water, the

  "Scotch whiskey" is practically restored.

  dre can be used in general for

  whiskey or as an additive to different foods.

ments.

EXAMPLE 3

  A corn starch emulsion is subjected to 2-stage hydrolysis using X-amylase, and the hydrolysis liquid, obtained by conducting the first liquefaction stage.

  with amylase (Crystase KD, from Daiwa Kasei K K)

  that the ED index of 1.7 is heated and boiled

  to inactivate the enzyme and perform the swelling and

  starch dispersion; during the second stage, the hy-

  drolysis is carried out with a new addition of O (-amylase (Crystase KD) up to an ED of 16.5, in order to obtain

  hydrolysed starch (water content 3%) having a concentration

  of 42.5% in alcoholic solubles

  saccharide position: 1.1% G 1, 5.7% G 2, 8.7% G 3, 7.3% G 4, 6.8% G 5, 13.7% G 6, 13.4% of G 7, 7.7% of G 8, and 35.6% of Gn. 100 kg of the hydrolysed starch obtained are then added to 125 kg of a brandy (V SOP). alcohol content of 46%; the resulting liquid mixture was heated to 55 ° C with a hot plate and then spray-dried at 72 ° C. to obtain about 152 kg of a brandy powder with an alcohol content of 34.3%.

(91% alcohol yield).

  When this brandy powder is dissolved in water, the fragrance of the resultant solution is practically no different from that of the original brandy, and this solution has

  low viscosity and good flavor The powder is excellent

  stable storage, particularly with regard to

  do moisture resistance and anti-property property

in mass.

EXAMPLE 4

  About 80 kg of the hydrolyzed starch of Example 1 (ED = 24, water content 5%) are dissolved in about 180 liters of water.

  8 g of magnesium sulphate, 50 g of mono-

  potash, 80 g yeast extract powder, 30 g peptone and 160 g baker's yeast (from

  Kaneka Yeast K K) and this solution is agitated and now

  naked at 30 1 C, with introduction of sterilized air at a rate of ml / minute / liter of solution. The culture is thus carried out for 45 hours, and the pH value is adjusted to 6.5 by sodium carbonate and the broth culture is heated

  at 90 ° C to achieve sterilization The resulting liquid

  is subjected to fading, deodorizing and

  and release, using activated charcoal and ion exchange resin, then spray-dried to obtain 68 kg of dry powder (2.5% water content). This powder has a critical soluble concentration. in 42% alcohol, an ED number of 14, a viscosity of 45 cps and a saccharide composition as follows: 1% G 1, 1.2% G 2, 6.4% G 3 , 9.2% of G 4, 9.9% of G 5, 8.4% of G 6, 8%

  G 7, 10.5% G 8, and 45.4% Gn.

  Then 38 kg of this powder is added to a free

  33 kg of dry flavored "sake" (16% alcohol content, 4% extract content and 80% water content)

  and 22 kg of alcohol at 92.4%, and it is heated to 60 C and then

  spray drying at a chamber temperature of 75 ° C

  to obtain about 63 kg of a refined, powdery sake

  slow, with an alcohol content of 37.5% (yield

93% alcohol).

  When this powder is dissolved in hot water,

  holds a refined sake-flavored "sake" drink with no sweetening power from the vehicle; the perfume of the refined sake of origin is sufficiently preserved and the

  drink has a good fragrance and is not viscous.

EXAMPLE 5

  A glutinous maize starch emulsion is subjected to 2-step hydrolysis using "amylase,

  Next step The first stage of hydrolysis, the

  quantization is carried out using Crystase KD (<< amylase) to an ED number of 1.8 and the liquid obtained is heated and boiled, in order to inactivate the enzyme and to achieve In the second stage, Crystase KD is again added and the hydrolysis is carried out to an ED number of 18, then the liquid is dried and a starch is obtained. hydrolyzed, of which the saccharide composition is: 1.5% G 1, 7.2% G 2, 11.5% G 3, 9.1% G 4, 8.3% G 5, 16, 8% of G 6, 13.5% of

  G 7, 5.5% of G 8 and 26.6% of Gn are treated, in the manner described above.

  in Example 4, 80 kg of this hydrolysed starch (

  5%) with yeast, to convert lower saccharides, such as glucose and maltose, and the treated starch is faded and released, then dried; approximately 70 kg of a dry powder containing 3% of water are obtained. This powder has a critical concentration of alcohol soluble of 47%; its saccharide composition is: 0% G 1, 0% G 2, 11.1% G 3, 10.1% G 4, 9.2%

  of G 5, 18.8% of G 6, 15% of G 7, 6.1% of G 8, and 29.7% of Gn

  The 70 kg of powder obtained are then added 50 kg of dark rum, with an alcohol content of 50%, produced in Jamalque, and the mixture is heated to 65 ° C. using

  of a hot plate and spray-dried at a time

  room temperature of 70 C; 117 kg of rum powder with an alcohol content of 40%, alcohol yield

94.2%.

  The rum powder obtained is well soluble in water, and the flavor of an aqueous solution of this powder does not differ substantially from that of the starting rum.

  practically no viscosity,

  In addition, this rum powder is very stable, especially with regard to the

  resistance to moisture absorption.

EXAMPLE 6

  One solution, consisting of 27.5 kg of virvid with 10% alcohol and 4% extract, 20 kg of 95% alcohol for drinking, 0.4 kg of tartaric acid, 0.1 kg of acid malic acid, 0.3 kg of citric acid, 0.1 kg of a wine perfume and 0.05 kg of a strawberry flavor, is mixed with 36 kg of a dry powder of a hydrolysed starch, obtained by conversion of the lower saccharides to yeast medium, as described in Example 4 The resulting liquid mixture is heated to C with a plate and spray-dried at a chamber temperature of 75 ° C; About 57 kg of a 33.5% alcohol powder are obtained. 50 kg of the powder thus obtained are then mixed homogeneously with 10 kg of crystallized sugar to form a wine cocktail powder. dissolves 40 g of this powder in 120 ml of cold water, the solubility in water is very good and the wine cocktail obtained, devoid of viscosity, is excellent in flavor and fragrance When sealing this wine cocktail powder in lined aluminum bags and stores it for a long time, it can be seen that

  the characteristics of stability, as not taken in mas-

  resistance to the absorption of moisture and

  flavor, are excellent, so it is confirmed

  that the powder obtained is interesting as a cocktail

taneous.

EXAMPLE 7

  A solution comprising 45 kg of a seasoning liqueur-

  soft gel ("mirin"), 8% extract and 20% alcohol, is mixed with 50 kg of dry powder of the hydrolysed starch, obtained in Example 5; the resulting liquid mixture is heated to 50 ° C with a hot plate and then spray-dried at a chamber temperature of 720 ° C; about 75 kg of "mirin" powder is obtained,

having an alcohol content of 31%.

EXAMPLE 8

  45 kg of a lemon essence containing 50% alcohol is added

  43.5 kg dry powder of the hydrolysed starch, obtained

  in Example 2, then dissolved, and the liquid mixture

  sultant is spray-dried at a chamber temperature of 750 ° C, to give about 65 kg of lemon oil powder The powder obtained has an alcohol content

  31.2% and water 2.5%; the flavor of a solution a-

  of this powder is almost identical to that

  lemon (liquid) essence of starting

  the powder is stored for a long time, its flavor is not modified; it can be used as an additive to tea or

instant juice.

EXAMPLE 9

  To a solution containing 64 kg of pepper tincture,

  % of alcohol, and 54 kg of water, are added 100 kg of

  Dry the hydrolyzed starch obtained in Example 3, and after dissolution, the resulting liquid mixture is spray dried at 780 C; about 150 kg of a powdered pepper dye is obtained at 32.3% alcohol. The powder obtained can be used effectively for different

sauce mixes.

EXAMPLE 10

  At 140 kg of a liquid containing 40% alcohol and 5% extract, ob-

  held by extraction of "bonito" dry with aqueous alcohol,

  125 kg of dry powder are added with a hydrolysed starch, obtained

  held in Example 3; after dissolution, the resulting solution is spray-dried at a chamber temperature of 780 ° C. to give about 182 kg of a bonito powder extract with an alcohol content of 27%. The perfume of this dry bonito is sufficiently preserved in the powder. obtained, as well as the alcohol component; after a

  long storage, it is observed that the powder remains sta-

  It therefore confirms that this powder can serve

  fictitious for different instant seasonings.

TABLE 1

viscosities

  té (cps) An enzyme hydrolyzed product A An enzyme hydrolyzed product B An acid hydrolyzed product A An enzyme hydrolyzed product E An acid hydrolyzed hydrolyzed product E An acid hydrolyzed product An enzyme hydrolyzed acid hydrolyzed product E ED 8.5 1 1

G 1 G 2

Tra 1,2 ce

0.6 3.1

3.9 4.4

2.6 4.5

4.5 6.8

7.1 7.4

8.5 8.4

  G 3 2.7 4.8 4.3, 2 4.9 7.8 8.5 G 4 2.7 4.2 4.2 4.6 4.8 8.2 9.8 G 5 2.3 4, 2 3.9 4.4, 1 8.0 11.2

G 6 G 7

4.4 5.7

6.3 7.0

3.2 3.0

6.8 6.7

4.7 4.9

7.2 6.8

, 8.1

  G 8, 3, 6.9, 3.3, 2, 9, 8.9, 9.5 Gn, 7, 62.9, 69.8, 0, 58.4, 38.6.

concentration

Critical

  % as alcohol-soluble products 36.5 38.0 37.3 49.8 57.7 61.2 N) Ln U r N a hydrolysed starch

(before splitting

  Fraction A Fraction B Fraction C

TABLE 2

viscosities

  t (cps) G 1 G 2 G 3 G 4 G 5 G 6 G 7 G 8 Gn ED

(%) (%) (%) (%) (%) (%) (%) (%) (%)

  7.3 6.8 6.4 5.7 5.6 5.3 5.5 6.6 50.8 21.5 38

  , 3 17.5 9.4 8.1 6.6 4.7 3.8 3.2 26.4 40

  1.8 2.1 7.8 8.0 7.7 8.2 9.4 11.5 43.5 16

  1.4 1.6 2.4 2.3 2.5 2.1 2.8 3.5 81.3 10

  Critical concentration in so much alcohol (%) t. '> Ln N (A ru

TABLE 3

  Case of the hydrolysed starch of Fraction A Quantity (parts) of alcohol per 100

parts of water.

Amount (parts) of starch, 5%

(21.5)

14.6%

(20.2)

, 6%

(15.9)

6.7%

(11.3)

17.9%

(28.0)

14.8%

(25,1)

11.7%

(21.8)

8.2%

(17.1)

19.6%

(37.1)

17.4%

(36.0)

14.5%

(33.0)

11.3%

(28.9)

hydrolyzed per 100 parts of water

19.3%

(41.9)

17.4%

(41.5)

14.7%

(38.7)

11.8%

(35.0)

18.5%

(45,1)

16.8%

(45,1)

14.3%

(42.5)

11.4%

(38.2)

* w O w N Ln -J 'r', L Ju DO L

TABLE 4

  Fraction B hydrolysed starch Quantity (parts) of alcohol per 100 parts of water Quantity (parts)

34.2%

(55.3%)

31.9%

(56.0%)

, 8%

(47.3%)

22.1%

(44.9%)

36.5%

(75.0%)

33.7%

(74.4%)

, 6%

(73.5%)

26.8%

(71.0%)

of amidorhydrolysed for 9%

(86.3%)

33.2%

(86.1%)

29.7%

(83.2%)

26.2%

(81.3%)

33.7%

(90.2%)

31.2%

(90.3%)

27.7%

(86.9%)

24.6%

(86.1%)

parts of water

31.9%

(94.0%)

29.3%

(93.3%)

26.5%

(92.6%)

23.7%

(92.9%)

r 1 Ln

TABLE 5

  Case of Fraction C hydrolyzed starch Amount (parts) of alcohol per 100 parts of water Amount (parts) white haze A

18.0%.

(23.1%)

white cloud A

18.8%

(29.8%)

  of hydrolysed starch per 100 parts of white turbid water A, 5%

(27.8%)

white disorder A, 8%

(21.1%)

spray drying

impossible to

because of the visco-

too high.

  It can not spray dry because of the viscosity too high. It is very cloudy white, 3%.

(37.9%)

white disorder B, 5%

(37.3%)

white disorder B

16.9%

(34.7%)

white disorder B

14.5%

(33.4%)

white disorder C, 5%

(46.5%)

27.3%

(59.6%)

white disorder C

26.0%

(58.4%)

27.8%

(74.7%)

white disorder C

24.0%

(61.9%)

26.6%

(83.0%)

-% 'Ln LY r OJ LAW

TABLE 6

  Case of the hydrolysed starch of the mixture of the fractions A and C in the proportion 1/3 Quantity (parts) of alcohol per 100 parts of water Quantity cloudy white B, 3%

(26,83)

white disorder C

21.4%

(32.3%)

  (parts) of hydrolysed starch per 100 parts of white turbid water B

19.8%

(31.7%)

white disorder B

24.2%

(47.7%)

white cloud A

16.3%

(29.5%)

white disorder B, 5%

(44.1%)

white cloud A

12.5%

(25.0%)

white disorder B

18.0%

(43.3%)

white disorder at 9.6%

(21.0%)

white disorder B

13.2%

(33.9%)

drying by atomization

impossible because of the

too high viscosity.

I he and, 6%

(46.8%)

22.4%

(45.7%)

27.5%

(63.1%)

23.6%

(59.8%)

0%, 9%

(68.6%)

22.7%

(67.1%)

white disorder C

23.0%

(67.5%)

21.4%

(71.7%)

Ln ru VI

TABLE 7

  Case of hydrolysed starch, before fractionation.

  Amount (parts) of alcohol per 100 parts of water Quantity

21.4%

(28.7%)

19.3%

(28.3%)

17.2%

(28.1%)

, 1%

(28.0%)

(parts)

28.6%

(51.9%)

26.0%

(51.1%)

22.4%

(47.8%)

18.9%

(44.9%)

of hydrolysed starch per 100

29.5%

(64.1%)

27.2%

(64.2%)

23.8%

(61.2%)

19.8%

(56.3%)

28.7%

(71.1%)

26.3%

(70.8%)

23.1%

(67.9%)

, 0%

(65.8%)

parts of water

27.8%

(77.0%)

, 6%

(77.3%)

23.0%

(76.5%)

, 3%

(75.9%)

P-J -A Pa Lnl (; ro

TABLE 8

  Case of Glucose, Maltose and Maltotriose (Alcohol: Water: Saccharide mixed in the proportions = 46: 54: 100) Saccharide Alcohol content Alcohol yield All adheres to the walls of the chamber, and the recovery of the powder is impossible Maltose 6, 0% Maltotriose

28.8%

  % 72% Adherence to the walls of the chamber, and the recovery rate

  powder is of the order of 70%.

  Adhesion to the walls of the chamber is observed and the resulting powder absorbs

relatively high humidity.

  Glucose Dry State CO L L L L 4 ro

Claims (8)

claims   Process for the preparation of powders containing alcohol which comprises mixing a hydrolysed starch with an aqueous solution containing alcohol and then drying the resulting liquid mixture by atomization, characterized in that the hydrolysed starch includes at   less than 50% of oligosaccharides having a degree of polymerisation   glucose level not exceeding 8, and not more than 10%   charides having equal glucose polymerization degree or less than 2.   Process according to Claim 1, characterized in that the hydrolysed starch does not comprise more than 5% of saccharides having a degree of glucose polymerisation equal to or less than 2.   Method according to one of claims 1 or 2,   characterized in that the hydrolysed starch is soluble in an aqueous solution of a 40% w / w alcohol, it being understood that, when a 25% aqueous solution of the hydrolysed starch is added to a 40% aqueous solution, % weight /   the weight of an alcohol (250 C), at the rate of 5%   the absorbance of the mixture at 600 nm after 5 minutes, is less than 0.5.   4 Process according to one of claims 1 to 3, characterized   in that the hydrolysed starch is obtained by with aqueous alcohol.   Process according to one of claims 1 to 3,   characterized in that the hydrolyzed starch is obtained according to a two-stage liquefaction process, which comprises   first-stage formation of a liquid starch; hydro-   lysed, whose ED index does not exceed 3, followed by   boiling and boiling of the hydrolysed liquid, then adding   second stage of (-amylase to this liquid, and hydrolysis   than at an ED index of about 12 to 20.   Process according to one of claims 1 to 3,   in that the hydrolysed starch used is obtained   by biochemical conversion, using a microorganism   especially yeast, saccharides with a degree of   lymerization equal to or less than 2, contained in a hydrolysed starch.   Method according to one of claims 1 to 6, characterized   in that the hydrolysed starch is added to a solution   water containing at least 40% w / w of alcohol,   100 to 200% of the water contained in the solution. aqueous composition containing this alcohol.   Process according to one of claims 1 to 7,   characterized in that the aqueous solution containing the alcohol is selected from among the mouth alcohols, spirits, mixed liquors, herbal spirits,   flavoring liquors such as perfumes, in particular   bind tincture of vanilla and orange essence, dyeing   spices, roots, aqueous alcohol extracts from   substances of approval of the table, as well as their ges.